Ethanol → HCID 178457032, Verbindung

HRID 1457484Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1457484
C(O)C.[OH-].[K+].[C:6]1([CH2:12][CH2:13][N:14]2[C:18]([Br:19])=[C:17]([C:20]([O:22]CC)=[O:21])[C:16]([N:25]([CH2:44][CH2:45][CH3:46])[CH2:26][C:27]3[CH:32]=[CH:31][C:30]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=4[C:39]4[NH:43][N:42]=[N:41][N:40]=4)=[CH:29][CH:28]=3)=[N:15]2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>O>[C:6]1([CH2:12][CH2:13][N:14]2[C:18]([Br:19])=[C:17]([C:20]([OH:22])=[O:21])[C:16]([N:25]([CH2:44][CH2:45][CH3:46])[CH2:26][C:27]3[CH:32]=[CH:31][C:30]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=4[C:39]4[NH:43][N:42]=[N:41][N:40]=4)=[CH:29][CH:28]=3)=[N:15]2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

Komponenten

5

Edukt 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 178457033HCID 178457033, Verbindung

Produkt 1

HCID 178457032HCID 178457032, VerbindungAusbeute 94,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

5 ml of ethanol, 5 ml of water and 226 mg of potassium hydroxide were added to 206 mg of N-[1-(2-phenylethyl)-4-ethoxycarbonyl-5-bromopyrazol-3-yl ]-N-[(2'-(1H-tetrazol-5-yl)-biphenyl-4-yl)methyl]-n-propylamine, and heated under reflux for 5 hours. Ethanol was distilled off under reduced pressure, and 10 ml of water were added to the reaction mixture, which was then made acidic with concentrated hydrochloric acid. The resultant was extracted with 50 ml of dichloromethane. After dried over magnesium sulfate, the extract was concentrated under reduced pressure and dried to obtain 185 mg of the intended compound as a pale yellow, amorphous solid.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 5 hours
  3. distillationEthanol was distilled off under reduced pressure, and 10 ml of water
  4. additionwere added to the reaction mixture, which
  5. extractionThe resultant was extracted with 50 ml of dichloromethane
  6. dry with materialAfter dried over magnesium sulfate
  7. concentrationthe extract was concentrated under reduced pressure
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-61bfc208f89a443a8da5d1f372ad0aea
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05846991

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